CN101643195A - Method and device for preparing colloid probe - Google Patents
Method and device for preparing colloid probe Download PDFInfo
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- CN101643195A CN101643195A CN200810118009A CN200810118009A CN101643195A CN 101643195 A CN101643195 A CN 101643195A CN 200810118009 A CN200810118009 A CN 200810118009A CN 200810118009 A CN200810118009 A CN 200810118009A CN 101643195 A CN101643195 A CN 101643195A
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Abstract
The invention discloses a method and a device for preparing a colloid probe, and relates to the probe technology. The colloid probe is prepared by adopting a three-dimensional translation stage to bi-directionally move and adjust the relative positions of a micro cantilever probe and colloid grains or optical adhesive droplets, carrying the micro cantilever probe through a rotary stage and a crossrod rack, adjusting the inclination angle of the micro cantilever probe and sticking the colloid grains to the back of the tip of a probe micro cantilever by using optical adhesive. The method and the device is suitable for preparing the colloid grain probe which uses an atomic force microscope to detect an interaction process of the grains and the surface (grains) so as to acquire a grain-surface (grain) acting force curve. The method and the device are characterized by simple and quick probe preparation operation, and strong practicability, and are suitable for batch manufacturing in a laboratory.
Description
Technical field
The present invention relates to the modification and the processing technology of preparing field of probe, is that a kind of microparticle that bonds on cantilever under Powerful Light Microscope is to prepare method and the device that the AFM mechanics sensor is a probe.
Background technology
AFM is that people such as Binnig was in invention in 1986.AFM energy high-resolution is surveyed the shape of atom and molecule, determine electricity, magnetic and the mechanical performance of body surface, becoming the conventional instrument that carries out microstructure observation, nanoscale processing in the fields such as physics, chemistry, biology, microelectronics and material science.Atomic force microscope probe is made up of several parts such as matrix, micro-cantilever and needle points, can divide bar shaped, " V " shape etc. several according to the shape of micro-cantilever.Probe tip is a key component of AFM, and it directly determines the resolution ratio of AFM, thereby influences microscopical application performance.Atomic force microscope probe is normally prepared by manufacturing procedures such as sputtering sedimentation, etchings by semi-conducting material, and traditional used semi-conducting material comprises silicon nitride, the various monocrystalline silicon etc. that mixes, and major part is the incorporate structure of micro-cantilever-needle point.The needle point that processes with the semi-conductor industry method, except that out-of-shape, its radius generally in several nanometers to tens nanometer range, thereby imaging resolution and observed result are subjected to needlepoint form and radius of curvature, affects bigger.During the last ten years, along with the continuous development and perfection of needle point modification with process technology, the resolution ratio of AFM and image quality have obtained very big improving, and its application has obtained very big expansion.Comprise that mainly self-assembled monolayer is modified atomic-force microscope needle-tip, biomolecule is modified atomic-force microscope needle-tip, electrochemical method modification needle tip of scanning tunnel microscope, nanometer tube modified atomic-force microscope needle-tip, or the like.Wherein, CNT is modified the focus that atomic-force microscope needle-tip becomes research recently.Physical property that CNT had and chemical property make it be suitable as very much the atomic-force microscope needle-tip material.
The colloid probe technology is that a micron-size spherical particles with smooth surface is bonded at a kind of microcosmic bonding making and the application technology of micro-cantilever end as mechanics sensor.It is the technology of preparing of a class specific use probe, and is widely used in surperficial force measurement.Write articles first at the Nature magazine in 1991 by people such as Ducker the earliest and deliver external at present more existing pertinent literatures reports [1-6].As a kind of probe modification and processing and preparing technology in scanning probe microscopy (SPM) observation technology, utilize the directly active force between the particle on measuring probe particle and the sample surfaces of colloid probe, and can be under the certain experiment condition of control its power component (as electric double layer power etc.) be carried out imaging and observe and measure, thereby simulation particle-particle interaction process, research colloidal solid thing microstructure and the mechanism of action thereof, and to relevant theoretical model estimate, the predictions and simulations experimental verification.Therefore, aspect the observational study of the DLVO Effect of Electric Double Layer power of from the teeth outwards adhesion of the microorganisms such as interaction, particle or bacterium between simulation natural water body colloidal solid, colloidal solid, the colloid probe technology will be brought into play its important function [7-8].
The preparation method of colloid probe mainly contains the two-wire method and cantilever moves method.Two-wire method (Dual-wire technique) is the method that Ducker et al uses the earliest, promptly with two very thin wires the microparticle of glue and several microns is transferred to the tip of cantilever respectively, carries out the microcosmic bonding of particle.Shortcoming is owing to utilize more weak capillary force, is difficult to use lametta that microparticle is shifted; The surface of easy destruction of metal wire and contaminate particulate; This method is damaged cantilever easily worse, and is not easy to find that cantilever damages.Cantilever moves method (cantilever-movingtechnique), and promptly single mobile cantilever comes first viscose glue to drip to the cantilever bottom surface, and then the bonding microparticle prepares the technology of probe.This method has than the two-wire method not to be used metal wire and has saved and sought suitable metal wire, and the plenty of time of the required cost of clean metal line, and has improved the agglomerability of cantilever and particle.But this method is not seen representational device and concrete method step.
List of references
[1]Ducker?W?A，Senden?T?J，Pashley?R?M.Direct?measurement?of?colloidal?forcesusing?an?atomic?force?microscope.Nature，1991，353：239-241.
[2]Ducker?W?A，Senden?T?J，Pashley?R?M.Measurement?of?Forces?in?Liquids?Usinga?Force?Microscope.Langmuir，1992，8(7)：1831-1836.
[3]Huntington?S，Nespolo?S.Precision?Attachment?of(Silica)Spheres?to?AFMCantilever?Tips.Microscopy?Today，2001，9(3)：32-33.
[4]Gan?Y.Attaching?Spheres?to?Cantilevers?for?Colloidal?Probe?ForceMeasurements：A?Simplified?Technique.Microscopy?Today，2005，13(6)：48-50.
[5]Gan?Y.A?review?of?techniques?for?attaching?micro-and?nanoparticles?toa?probe’s?tip?for?surface?force?and?near-field?optical?measurements.Reviewof?Scientific?Instruments，2007，78：081101.
[6]John?Ralston，Ian?Larson，Mark?W.Rutland，Adam?A.Feiler?and?Mieke?Kleijn.Atomic?Force?Microscopy?and?Direct?Surface?Force?Measurements.Pure?Appl.Chem.，2005，77(12)，2149-2170.
[7]Raiteri?R，Preuss?M，Grattarola?M，Butt?H-J.Preliminary?results?on?theelectrostatic?double-layer?force?between?two?surfaces?with?high?surfacepotentials.Colloids?and?Surfaces?A，1998，136(1-2)：191-197.
[8]Wijting?W?K，Knoben?W，Besseling?N?A?M，Leermakers?F?A?M，Stuart?M?A?C.Depletion?interaction?measured?by?colloidal?probe?atomic?force?microscopy.Phys.Chem.Chem.Phys.，2004，6：4432-4439.
Summary of the invention
The purpose of this invention is to provide a kind of colloid probe preparation method and device, this preparation method rapidly and efficiently, and effect is more satisfactory.
For achieving the above object, technical solution of the present invention is:
A kind of method for preparing colloid probe, it comprises the following steps:
(A) earlier mica sheet is bondd through sheet glass and bronze medal post upper end with two-sided tape, will be put in the liquid dispersed agent as the particle of needle point,, pipette mixed solution with liquid-transfering gun with ultrasonic dispersion≤5 minute, be added drop-wise on the mica sheet of copper capital end, standby after the air dry;
(B) modulated optical glue droplet: earlier sheet glass is bondd with two-sided tape and another copper post upper end, the ratio of bicomponent epoxy resin optical cement in 1: 1 dripped on the sheet glass of another copper capital end, it is standby that the back is mixed well in mixing;
(C) probe is installed on the Probe clip, then Probe clip is installed in the support termination of the second three-dimensional mobile platform, probe is placed under the light microscope observes, find the cantilever of probe, and observe cantilever whether incompleteness is arranged, to determine and to use;
(D) the copper post that has the optical cement droplet that will prepare in (B) step is placed on the plane of the first three-dimensional mobile platform;
(E) adjust the relative position of first, second three-dimensional mobile platform, make another copper post and probe close, and under light microscope, observe, the relative altitude of probe cantilever and another copper capital end optical cement droplet, utilize the capillary tension of liquid then to the surface, in the most advanced and sophisticated bottom surface of probe cantilever, be stained with an optical cement droplet;
(F) unclamp hold-down nut, the upset Probe clip, the nut that is tightened again makes progress the bottom surface of cantilever, and whether the size and location of observing optical cement droplet on the cantilever tip under light microscope are suitable;
(G) adjust hold-down nut, again Probe clip is overturn, remove another copper post that has the optical cement droplet, lay a bronze medal post that has microsphere particle that makes in (A) step;
(H) adjust the relative position of first, second three-dimensional mobile platform, make a bronze medal post and probe close, and under light microscope, observe, adjust the height that cantilever tip glue drips, and at the suitable microsphere particle that uses of mica sheet surface searching, in the most advanced and sophisticated bottom surface of cantilever, utilize the viscosity of existing glue, be stained with the microsphere particle of choosing;
(I) adjust hold-down nut, the upset Probe clip makes progress the bottom surface of cantilever, observes the microsphere particle that bonds on the cantilever under light microscope, whether in cantilever tip central authorities' symmetric position and particle surface situation, comprehensively judge colloid needle point bonding performance according to microsphere particle;
(J) probe of bonding microsphere particle on the cantilever is moved on to infrared roasting lamp under toasted≤1 hour, the optics hot-setting adhesive is solidified, colloid probe completes.
The described method for preparing colloid probe, its described particle is the silicon microballoon, the pressed powder of polystyrene spheres, colloid or latex particle or microsphere particle.
The described method for preparing colloid probe, its described liquid dispersed agent is water or ethanol; The used binding agent of bonding microsphere particle is for the two component optical cements of epoxide resin type, as Epotek 377.
The described method for preparing colloid probe is fit to the microsphere particle that uses in its described (H) step, for diameter less than 30 μ m, the best is the particle of 1～5 μ m.
The described method for preparing colloid probe; it adopts the relative position of the two cover two-way mobile adjusting probe cantilevers of independently three-dimensional mobile platform and microsphere particle or optical cement droplet; the control microcosmic moves bonding or contact process flexibly, makes the probe manufacturing faster and more convenient operation.
A kind of described method institute operative installations for preparing colloid probe comprises computer, operating desk, light microscope, CCD, outer light source, coaxial light source, two three-dimensional mobile platforms, two copper posts, Probe clip and infrared roasting lamps; Wherein,
Two three-dimensional mobile platforms, outer light source and support on square operating desk, have been fixed, support is provided with light microscope in vertical direction, the optical microphotograph lens head is downward, two three-dimensional mobile platforms lay respectively at both sides under the light microscope, outer light source is positioned at light microscope one side, and its light beam shines in microscope camera lens lower area;
Be furnished with CCD, coaxial light source in the light microscope lens barrel, CCD is electrically connected with computer through lead; Coaxial light source and outer light source change over the illumination condition of picture together;
Two copper post lower ends are furnished with permanent magnet, and planar central has the irony screw on the first three-dimensional mobile platform, to cooperate the fixed copper post with permanent magnet; The second three-dimensional mobile platform is provided with turntable, and turntable is connected with a support, and this support intersects and to be socketed with another support, the intersection by hold-down nut with two stands can loosen affixed;
Be provided with external screw thread in another support termination, the Probe clip sidewall is provided with blind hole, is provided with internal thread in the blind hole, and both match Probe clip is fixed in another support termination;
Probe clip and probe are dismountable affixed.
Described operative installations, the turntable of its described second three-dimensional mobile platform indicates scale, makes another riding one angle by the screw rod adjustment, is beneficial to the probe bonded particulate.
Described operative installations, its described another riding one angle that makes, this angle≤15 °.
Described operative installations, its described Probe clip is the block of a band groove, and groove axially is provided with, and is positioned at the bottom surface, and groove one end is open, other end sealing, the blind end lateral wall is provided with blind hole, is provided with internal thread in the blind hole;
The groove inner top surface is provided with the groove of putting probe, and the groove of putting probe axially is provided with; The close blind end of groove inner top surface is provided with the screw of the clip of perforation, is furnished with the reed fixed screw in the screw, after the reed fixed screw passes spring leaf, is bolted in the groove; Spring leaf axially is provided with, and is positioned at the groove of putting probe, spring leaf and probe dismountable affixed after, put probe in the groove of putting probe, and the head of probe stretched out in outside the groove;
Probe clip end face center is provided with a switch of propping spring leaf.
Described operative installations, the spring leaf of its described Probe clip are bar shaped, and it is near the local hollow out of groove open end, and the spring leaf lamellar body has curvature.
Described operative installations, its described probe are to have the finished product probe of needle point or do not have the needle point cantilever probe; Its cantilever is " V " shape or clavate.
The present invention has compared following advantage than existing with the gluing method for preparing needle point of getting of chemistry: (1) has adopted Powerful Light Microscope to connect computer by CCD, carries out real time and on line monitoring, is more conducive to observe and operation.(2) Powerful Light Microscope has adopted coaxial light source and outer light source light path system, has improved the contrast and the observability energy of imaging; Powerful Light Microscope adopts adjustable multiplying power camera lens, has improved local observing effect.(3) adopt three-dimensional move operation platform and turntable to adjust the angle of inclination of probe, make probe be more conducive to the sticking particle of getting.(4) made Probe clip, the groove of design and the spring clip of local hollow out have been protected the not cantilever of operating side of matrix, and operability is strengthened.
The present invention makes simple and quick, and is practical, is applicable to that the laboratory makes in batches.
Description of drawings
Fig. 1 is the schematic diagram of colloid probe preparation facilities of the present invention;
Fig. 2 (a) and (b), (c), (d) are the schematic diagrames of colloid probe preparation process of the present invention;
Fig. 3 is the schematic diagram of the three-dimensional mobile platform upper bracket of local A among Fig. 1;
Fig. 4 is the schematic diagram in Probe clip of the present invention front;
Fig. 5 is the schematic diagram at the Probe clip of the present invention back side.
The specific embodiment
Below in conjunction with the drawings and specific embodiments the present invention is further described.
See also Fig. 1, Fig. 3, Fig. 1 is the schematic diagram of colloid probe preparation facilities, and Fig. 3 is the schematic diagram of local A among Fig. 1.Turntable 9, copper post 10, Probe clip 18, probe 19, hold-down nut 20, support 21, support 22.
A kind of described method institute operative installations for preparing colloid probe comprises computer 1, operating desk 2, light microscope 3, CCD4, outer light source 5, coaxial light source 6, two 7,8, two copper posts 10 of three-dimensional mobile platform, Probe clip 18 and infrared roasting lamps (not illustrating among the figure); Wherein,
Fixed two three-dimensional mobile platforms 7,8 and support on square operating desk 2, support is provided with light microscope 3 in vertical direction, and the optical microphotograph lens head is downward, and two three-dimensional mobile platforms 7,8 lay respectively at both sides under the light microscope 3; Outer light source 5 device boxes are put in square operating desk 2 sides, and light source probe is positioned at light microscope 3 one sides, and its light beam shines in microscope camera lens lower area;
Be furnished with CCD4, coaxial light source 6 in the light microscope lens barrel, CCD4 is electrically connected with computer 1 through lead; Coaxial light source 6 and outer light source 5 change over the illumination condition of picture together.
Two copper post 10 lower ends are furnished with permanent magnet, and planar central has the irony screw on the first three-dimensional mobile platform 7, to cooperate fixed copper post 10 with permanent magnet; The second three-dimensional mobile platform 8 is provided with turntable 9, and turntable 9 is connected with a support 21, and this support 21 intersects and is socketed with another supports 22, the intersection by hold-down nut 20 with two stands 21,22 can loosen affixed;
Be provided with external screw thread in another support 22 terminations, Probe clip 18 sidewalls are provided with blind hole (not illustrating among the figure), are provided with internal thread in the blind hole, and both match Probe clip 18 is fixed in another support 22 terminations;
The turntable 9 of the second three-dimensional mobile platform 8 indicates scale, makes tilt≤15 ° angle of another support 22 by the screw rod adjustment, is beneficial to probe 19 bonded particulates.
Seeing also Fig. 4, is the schematic diagram in Probe clip 18 fronts; Wherein, have Probe clip front 23, reed fixed screw 24, spring leaf 25, reed openwork part 26, put the groove 27 of probe.
Seeing also Fig. 5 is the schematic diagram at Probe clip 18 back sides, the screw 29 of the Probe clip back side 28, clip, props the switch 30 of spring leaf, the groove 31 of Probe clip.
28 centers, the Probe clip back side are provided with a switch 30 of propping spring leaf.
See also Fig. 2 (a) and (b), (c), (d), it is the schematic diagram of colloid probe preparation process of the present invention, wherein, have that cantilever 12, glue 13, copper post 14, the glue of optical microphotograph camera lens part 11, probe drip 15, the particle 16 on the copper post, the particle 17 on the cantilever.Probe 19 is to have the finished product probe of needle point or do not have the needle point cantilever probe; Its cantilever 12 is " V " shape or clavate.
A kind of method for preparing colloid probe of the present invention comprises following steps:
(A) will be put in the liquid dispersed agent as the particle of needle point,, pipette mixed solution, be added drop-wise on the mica sheet of copper post air dry with liquid-transfering gun with ultrasonic dispersion≤5 minute; Mica sheet bonds through sheet glass and copper post with two-sided tape.
(B) modulated optical glue droplet: the ratio of bicomponent epoxy resin optical cement in 1: 1 dripped on the sheet glass of copper post, mix with thin wire and mix well.
(C) probe is installed on the Probe clip 18 (referring to Fig. 3), then Probe clip is installed on the support 22 (referring to Fig. 3) of three-dimensional mobile platform 8, under the observation of Powerful Light Microscope 11, finds the cantilever 12 of probe, and observe cantilever whether incompleteness is arranged, to determine and can use.
(D) will be placed on the platform of three-dimensional mobile platform 7 at the copper post that has the optical cement droplet in (B) step;
(E) under the observation of Powerful Light Microscope 11, adjust the height of cantilever and optical cement droplet 13, utilize the capillary tension of liquid to the surface, in the most advanced and sophisticated bottom surface of cantilever, be stained with an optical cement droplet (a) referring to Fig. 2;
(F) unclamp nut 20, upset Probe clip 18 screws nut 20, the bottom surface that makes cantilever upwards, whether the size and location of observing optical cement droplet 15 on the cantilever suitable (referring to Fig. 2 b).
(G) adjust nut 20, again Probe clip is overturn, remove the copper post that has the optical cement droplet, lay the copper post that has microsphere particle that makes in (A) step;
(H) under the observation of Powerful Light Microscope 11, adjustment cantilever 12 and glue drip 15 height, and seek the microsphere particle that is fit to use on the mica sheet surface, in the most advanced and sophisticated bottom surface of cantilever, utilize the viscosity of glue, are stained with this microsphere particle (referring to Fig. 2 c);
(I) adjust nut 20, upset Probe clip 18 makes progress the bottom surface of cantilever, observes the microsphere particle that bonds on the cantilever, whether in cantilever tip central authorities' symmetric position and particle surface situation, comprehensively judge colloid needle point bonding performance (referring to Fig. 2 d) according to microsphere particle.
(J) probe with bonding microsphere particle on the cantilever toasted≤1 hour under infrared roasting lamp, and the optics hot-setting adhesive is solidified, and colloid probe completes.
It is no needle point micro-cantilever silicon nitride or silicon semiconductor probe material that the present invention prepares the colloid probe material therefor.Use the cylindrical, copper post of diameter as 8mm, base the is bonding magnet of a fritter same diameter conveniently utilizes magnetic to be fixed on the three-dimensional mobile platform.Use two-sided tape that the square thin glass sheet of 1cm * 1cm is adhered on the copper post, the mica sheet that will handle adheres on the thin glass sheet with double faced adhesive tape again, with adhesive tape mica sheet is carried out cleavage then, obtains fresh smooth mica surface.
Colloidal solid adopts the diameter of buying 5,10, the silicon microballoon that 20 μ m do not wait.Be diluted to certain density solution, adopt high frequency ultrasound, colloidal solid is uniformly dispersed.With 10 μ L liquid-transfering guns, the particle dispersion liquid of suitable concentration is transferred on the mica surface.After the air dry, open coaxial light source, the multiple of zoom microscope is adjusted the copper post height that loads particle step by step, finds the particle that is fit to use.
Powerful Light Microscope has adopted coaxial light source and outer light source light path system, and the light microscope lens set adopts WA 121204 models, 20 * infinity camera lens.Use 14 inches LCDs, during full screen display, maximum amplification is: 20 * 1.5 * 3 * 14=1260.Light-source system adopts the 150W cold light source, is a kind of source of parallel light.Axis light is more conducive to imaging, and outer light source makes particle have more third dimension, thereby, improved the contrast and the observability energy of imaging.The eyepiece of Powerful Light Microscope upper end is installed CCD and is connected on the image pick-up card of computer.CCD adopts " 1/3 " Color CCD Camera, 470TV Lines, and (CCIR EIA), has the AWB function to the PAL video standard for PAL, NTSC.Use PCI TV Card image pick-up card, software use V3.3 version software (GADMEI,
Www.gadmei.com).Realize online observation, and can take pictures, recorded video.Perfect imaging system, the convenient observation improved operability.
The optics hot-setting adhesive adopts the two component optical cements of Epotek 377 epoxy resins of epoxy technologies (EpoTek) company, this glue is divided into A, B component, A component useable glass bottle or plastic bottle are preserved (epoxy resin principal component) .B component and should be transferred in the vial, keep in Dark Place.A and B two mixture ratio examples 1: 1,24 hours normal temperature cure time, under the heating condition 7-8 minute promptly curable, this optical cement is a hot-setting adhesive.
Turntable can be adjusted probe and tilt arbitrarily angled.About becoming with horizontal plane about 15 degree, can make probe be more conducive to the sticking particle of getting greatly.
The three-dimensional manipulating platform realizes that the three-dimensional two-way of cantilever, glue and colloidal solid moves.Improved the flexibility of operation.The minimum scale of operation screw rod moving displacement is: 0.01mm, can satisfy the needs of operation.
The Probe clip of self manufacture, the groove of design and the spring clip of local hollow out have been protected the not cantilever of operating side of matrix, and operability is strengthened.
The present invention promptly uses the laboratory to develop device voluntarily for cantilever moves the improvement and the raising method of method, adopts the gluing colloidal solid of getting of optics.The inventive method adopts Powerful Light Microscope-CCD-computer real-time monitoring system, utilizes the three-dimensional manipulating platform, realizes that the two-way three-dimensional of cantilever, glue and colloidal solid moves.Use spherical microparticle as needle point; Spherical needle point can better be simulated the active force between the spheric granules, simple shape, and the convenient mathematical method of using is calculated, and is more conducive to the explanation of measurement result and the repeatability that realizes experiment.Powerful Light Microscope has adopted coaxial light source and outer light source light path system, has improved the contrast and the observability energy of imaging.Thereby, can widen range of application more widely for AFM.Device of the present invention can be handled diameter greater than 1 micron microballoon, and is easy to operate, practical; Can be used as the servicing unit of other method of modifying.
Embodiment (one):
(1) diameter 10 μ m silicon microballoons is distributed in the aqueous solution,, uses liquid-transfering gun to pipette certain quantity solution, be added drop-wise on the mica sheet of copper post 10 air dry with ultrasonic dispersion 5 minutes.Mica sheet bonds through sheet glass and copper post with two-sided tape.Observe for 11 times in Powerful Light Microscope, find the microballoon that is fit to use.
(2) modulation Epotek 377 optical cements drip.With the bicomponent epoxy resin optical cement, drip on a small quantity to the sheet glass of copper post in 1: 1 ratio, mix with thin wire and to mix well.
(3) probe is installed on the Probe clip 18, then Probe clip 18 is installed on the support 22 of three-dimensional mobile platform 8.Under the observation of Powerful Light Microscope 11, find the cantilever 12 of probe, whether can observing cantilever has incompleteness, to determine and use.
(4) the copper post that glue drips that has in (2) step is placed on the platform of three-dimensional mobile platform 7.
(5) adjust the height that cantilever and glue drip, under the observation of Powerful Light Microscope 11,, be stained with a droplet glue (a) referring to Fig. 2 in the most advanced and sophisticated bottom surface of cantilever.
(6) upset Probe clip 18 makes progress the bottom surface of cantilever.Whether the size and location of observing optical cement droplet 15 on the cantilever suitable (referring to Fig. 2 b).
(7) again Probe clip is overturn, remove and have the copper post that glue drips, lay the copper post that has microsphere particle that makes in (1) step.
(8) adjust the height that cantilever and glue drip, under the observation of Powerful Light Microscope,, utilize the viscosity of glue, be stained with microballoon 16 (referring to Fig. 2 c) in the most advanced and sophisticated bottom surface of cantilever.
(9) upset Probe clip makes progress the bottom surface of cantilever.Observe the microsphere particle 17 that bonds on the cantilever, whether in cantilever tip central authorities' symmetric position and particle surface situation, comprehensively judge colloid needle point bonding performance (referring to Fig. 2 d) according to microsphere particle
(10) under infrared roasting lamp, toasted about one hour, hot-setting adhesive is solidified.Make the silicon dioxide microsphere colloid probe.
Embodiment (two):
(1) diameter 5 μ m silicon microballoons is distributed in the aqueous solution,, uses liquid-transfering gun to pipette certain quantity solution, be added drop-wise on the mica sheet of copper post 10 air dry with ultrasonic dispersion 5 minutes.Mica sheet bonds through sheet glass and copper post with two-sided tape.Adjusting microscopical multiplying power for 11 times in Powerful Light Microscope is 3.5, observes and find the microballoon that is fit to use.
In other steps, be, when using Powerful Light Microscope, all will note in good time adjusting microscopical multiplying power, be amplified to suitable multiple step by step and carry out microparticle the bond observation and the manipulation of process with different in embodiment ().
Claims (12)
1. a method for preparing colloid probe is characterized in that, comprises the following steps:
(A) earlier mica sheet is bondd through sheet glass and bronze medal post upper end with two-sided tape, will be put in the liquid dispersed agent as the particle of needle point,, pipette mixed solution with liquid-transfering gun with ultrasonic dispersion≤5 minute, be added drop-wise on the mica sheet of copper capital end, standby after the air dry;
(B) modulated optical glue droplet: earlier sheet glass is bondd with two-sided tape and another copper post upper end, the ratio of bicomponent epoxy resin optical cement in 1: 1 dripped on the sheet glass of another copper capital end, it is standby that the back is mixed well in mixing;
(C) probe is installed on the Probe clip, then Probe clip is installed in the support termination of the second three-dimensional mobile platform, probe is placed under the light microscope observes, find the cantilever of probe, and observe cantilever whether incompleteness is arranged, to determine and to use;
(D) the copper post that has the optical cement droplet that will prepare in (B) step is placed on the plane of the first three-dimensional mobile platform;
(E) adjust the relative position of first, second three-dimensional mobile platform, make another copper post and probe close, and the relative altitude of under light microscope, observing probe cantilever and another copper capital end optical cement droplet, utilize the capillary tension of liquid then to the surface, in the most advanced and sophisticated bottom surface of probe cantilever, be stained with an optical cement droplet;
(F) unclamp hold-down nut, the upset Probe clip, the nut that is tightened again makes progress the bottom surface of cantilever, and whether the size and location of observing optical cement droplet on the cantilever tip under light microscope are suitable;
(G) adjust hold-down nut, again Probe clip is overturn, remove another copper post that has the optical cement droplet, lay a bronze medal post that has microsphere particle that makes in (A) step;
(H) adjust the relative position of first, second three-dimensional mobile platform, make a bronze medal post and probe close, and under light microscope, observe, adjust the height that cantilever tip glue drips, and at the suitable microsphere particle that uses of mica sheet surface searching, in the most advanced and sophisticated bottom surface of cantilever, utilize the viscosity of existing glue, be stained with the microsphere particle of choosing;
(I) adjust hold-down nut, the upset Probe clip makes progress the bottom surface of cantilever, observes the microsphere particle that bonds on the cantilever under light microscope, whether in cantilever tip central authorities' symmetric position and particle surface situation, comprehensively judge colloid needle point bonding performance according to microsphere particle;
(J) probe of bonding microsphere particle on the cantilever is moved on to infrared roasting lamp under toasted≤1 hour, the optics hot-setting adhesive is solidified, colloid probe completes.
2. the method for preparing colloid probe according to claim 1 is characterized in that, described particle is the silicon microballoon, the pressed powder of polystyrene spheres, colloid or latex particle or microsphere particle.
3. the method for preparing colloid probe according to claim 1 is characterized in that, described liquid dispersed agent is water or ethanol; The used binding agent of bonding microsphere particle is for the two component optical cements of epoxide resin type, as Epotek 377.
4. the method for preparing colloid probe according to claim 1 is characterized in that, is fit to the microsphere particle of use in described (H) step, is the particle of diameter less than 30 μ m.
5. the method for preparing colloid probe according to claim 1 is characterized in that, is fit to the microsphere particle of use in described (H) step, and the best is the particle of 1～5 μ m.
6. the method for preparing colloid probe according to claim 1; it is characterized in that; adopt the relative position of the two cover two-way mobile adjusting probe cantilevers of independently three-dimensional mobile platform and microsphere particle or optical cement droplet; the control microcosmic moves bonding or contact process flexibly, makes the probe manufacturing faster and more convenient operation.
7. a method institute operative installations for preparing colloid probe as claimed in claim 1 comprises computer, operating desk, light microscope, CCD, outer light source, coaxial light source, two three-dimensional mobile platforms, two copper posts, Probe clip and infrared roasting lamps; It is characterized in that,
Two three-dimensional mobile platforms, outer light source and support on square operating desk, have been fixed, support is provided with light microscope in vertical direction, the optical microphotograph lens head is downward, two three-dimensional mobile platforms lay respectively at both sides under the light microscope, outer light source is positioned at light microscope one side, and its light beam shines in microscope camera lens lower area;
Be furnished with CCD, coaxial light source in the light microscope lens barrel, CCD is electrically connected with computer through lead; Coaxial light source and outer light source change over the illumination condition of picture together;
Two copper post lower ends are furnished with permanent magnet, and planar central has the irony screw on the first three-dimensional mobile platform, to cooperate the fixed copper post with permanent magnet; The second three-dimensional mobile platform is provided with turntable, and turntable is connected with a support, and this support intersects and to be socketed with another support, the intersection by hold-down nut with two stands can loosen affixed;
Be provided with external screw thread in another support termination, the Probe clip sidewall is provided with blind hole, is provided with internal thread in the blind hole, and both match Probe clip is fixed in another support termination;
Probe clip and probe are dismountable affixed.
8. operative installations according to claim 7 is characterized in that the turntable of the described second three-dimensional mobile platform indicates scale, makes another riding one angle by the screw rod adjustment, is beneficial to the probe bonded particulate.
9. operative installations according to claim 8 is characterized in that, described another riding one angle that makes, this angle≤15 °.
10. operative installations according to claim 7 is characterized in that, described Probe clip is the block of a band groove, and groove axially is provided with, and is positioned at the bottom surface, and groove one end is open, other end sealing, and the blind end lateral wall is provided with blind hole, is provided with internal thread in the blind hole;
The groove inner top surface is provided with the groove of putting probe, and the groove of putting probe axially is provided with; The close blind end of groove inner top surface is provided with the screw of the clip of perforation, is furnished with the reed fixed screw in the screw, after the reed fixed screw passes spring leaf, is bolted in the groove; Spring leaf axially is provided with, and is positioned at the groove of putting probe, spring leaf and probe dismountable affixed after, put probe in the groove of putting probe, and the head of probe stretched out in outside the groove;
Probe clip end face center is provided with a switch of propping spring leaf.
11. operative installations according to claim 10 is characterized in that, the spring leaf of described Probe clip is bar shaped, and it is near the local hollow out of groove open end, and the spring leaf lamellar body has curvature.
12., it is characterized in that described probe is to have the finished product probe of needle point or do not have the needle point cantilever probe according to claim 7,10 or 11 described operative installations; Its cantilever is " V " shape or clavate.
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